CN105647227A - Method for separating red pigment from yellow pigment of paprika red pigment - Google Patents
Method for separating red pigment from yellow pigment of paprika red pigment Download PDFInfo
- Publication number
- CN105647227A CN105647227A CN201511017918.8A CN201511017918A CN105647227A CN 105647227 A CN105647227 A CN 105647227A CN 201511017918 A CN201511017918 A CN 201511017918A CN 105647227 A CN105647227 A CN 105647227A
- Authority
- CN
- China
- Prior art keywords
- pigment
- leachate
- liquid
- red pigment
- extracting method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for separating red pigment from yellow pigment of paprika red pigment. The method comprises the following steps: drying, crushing, pelletizing and extracting paprika to obtain pigment lixivium; removing a spicy substance from the pigment lixivium, and then performing chromatographic separation by adopting wet process continuous sample feeding to separately obtain two kinds of eluent; concentrating the two kinds of eluent to obtain paprika yellow pigment and the paprika red pigment. According to the method, production efficiency of the paprika red pigment is obviously increased in a manner of liquid-liquid continuous extraction for spicy substance removal, and meanwhile, the deficiency of the chromatographic separation in industrial production of the paprika red pigment is made up by adopting a way of wet process continuous sample feeding of pigment extract, and a new direction is opened for industrial development of paprika red pigment.
Description
Technical field
The present invention relates to food additive field, the method being specifically related to the yellow red separation of a kind of capsicum red pigment.
Background technology
Capsicum red pigment (Paprikaredpigment) is the natural red colouring matter extracted from ripe Fructus Capsici peel, key component is capsorubin (Capsanthin), capsorubin (Capsorubin), beta-carotene (��-carotene) and cryptoxanthin (zeaxanthin) etc., its colored intensity is 10 times of other pigments, extensively in industries such as food, beverage, cosmetics and medicine, it it is the best A class red pigment generally acknowledged in the world. Capsicum red pigment is the part in Fructus Capsici in hunting pink. Because its tone is bright-coloured, safe and reliable and has pharmacological action, not being to be considered only as a kind of desirably natural food Agent, and be widely used in pharmaceutical industry, coating such as tablet is painted, has important researching value.
In different capsicum variety mature fruits, the content of carotenoid differs greatly, in different ripening stages pepper fruit, carotenoid total amount, Red carotenoids (capsorubin, capsorubin, hidden capsanthin) content and chlorophyllous content all vary widely, from the result initial stage to fruit full maturity, carotenoid content and Red carotenoids amount increase by 66 times and 124 times respectively, and chlorophyll content to time ripe close to zero, the red ratio with yellow also increases to 1.34 from 0.22.
The main preparation technology of traditional capsicum red pigment is by pepper drying, pulverizing, solvent extraction method is adopted to obtain the crude extract of capsicum red pigment, then adopt alkali liquor or ethanol equal solvent to extract elimination spicy substance again, and distill out the capsicum red pigment that solvent therein obtains refining.
CN102746696A discloses the extracting method of a kind of capsochrome, with Fructus Capsici for raw material, size-reduced, extract, layering, prepare after the decompression step such as distillation.
CN104672947A discloses the extraction process of a kind of high-purity stability Fructus Capsici pigment, and described extraction process comprises the following steps: a, pretreatment of raw material; B, drying squeezing c, flocculate and clarify; D, filtration e, lixiviate filtrate; F, making 40 color valency pigments, wherein adopt chitosan as Old Region, make product yield relatively improve, production cost reduces.
CN1045114A discloses a kind of method extracting pigment and Capsaicin from Fructus Capsici, it it is critical only that with the pigment in the aqueous extracting capsicum powder of ethanol and Capsaicin, extract is through being distilled off ethanol, stratification obtains oleo resin capsicum and Capsaicin solution, extracting the Capsaicin of residual in oils and fats with the aqueous washing of ethanol again, the second alcohol and water through being distilled off in Capsaicin solution obtains Capsaicin.
JP2004-302541A discloses a kind of Capsochrome preparation, and it is the O/W emulsion composition oil phase containing capsochrome and oil loving food emulsifying agent and the aqueous phase emulsifying containing hydrophilic macromolecular compounds and water formed.
" in microwave radiation exaraction Capsicum chinense the technical study of capsaicin and flavochrome ", Dong Liwei etc., Hainan Normal University's journal (natural science edition), 26th volume the 4th phase, in December, 2013, adopt microwave assisting method to extract capsaicin and flavochrome from the Capsicum chinense that Hainan is cultivated, and with HPLC and ultraviolet spectrophotometer, capsaicin and Yellow pigment content are measured respectively, investigate the optimal extract process of capsaicin and flavochrome with orthogonal experiment.
But, include the capsicum red pigment component that the existing technology of preparing of above-mentioned document obtains excessively complicated, red, the orange and yellow three kinds of components wherein comprised can produce larger difference with different sources, maturation time and preparation technology, can cause that the reddish yellow ratio of capsicum red pigment is unstable, thus having influence on the quality of capsanthin product, not there is general applicability. Mentioning that capsicum red pigment is extracted concentrated solution and refines by the method adopting silica gel column chromatography although also having in bibliographical information both at home and abroad, utilizing the single solvent such as petroleum ether and acetone or two kinds of combination solvents to carry out washing and obtain more single capsanthin product. But, above-mentioned involved method, due to its intrinsic defective workmanship, is suitable only for the separation of laboratory lab scale sample, and the production that cannot meet workshop under existence conditions is amplified.
This area needs a kind of method that applicable industrial scale carries out the yellow red separation of capsicum red pigment.
Summary of the invention
In view of this, it is contemplated that overcome of the prior art above not enough, it is provided that the method for the yellow red separation of a kind of capsicum red pigment, including:
Step (1): Fructus Capsici granule and leaching agent are mixed in continuous way infuser, obtains pigment leachate;
Step (2): mixed in liquid-liquid continuous extraction device with alcohols solvent by described pigment leachate, slough spicy substance, obtains pigment and takes off peppery leachate;
Step (3): described de-peppery pigment leachate and saturated aqueous common salt are mixed in liquid-liquid continuous extraction device, sloughs alcohols solvent residual;
Step (4): the pigment leachate obtained after elimination alcohols solvent is directly gone up silicagel column and carries out chromatography collection port effluent;
Step (5): treat that silicagel column absorption is saturated, adopt alkane solvents to carry out eluting, eluent merges with the described port collection liquid of step (4) and concentrates to obtain Fructus Capsici flavochrome;
Step (6): adopt acetone that described silicagel column is carried out eluting, eluent concentration obtains capsicum red pigment.
Preferably, described leaching agent is the alkane containing 4��7 carbon;
Preferably, described infuser is flat rotary extractor, loop type extractor, satellite type infusion device or crawler type infuser;
Preferably, described alcohols solvent is the alcohols solvent containing 1��4 carbon;
Preferably, described pigment leachate and alcohols solvent mixed proportion are 1:1��7;
Preferably, described de-peppery pigment leachate and saturated aqueous common salt mixed proportion are 1:1��7;
Preferably, described alkanes eluant is the alkane containing 4��7 carbon;
Preferably, described alkanes eluant and silicagel column are 2��6:1 by volume;
Preferably, described acetone eluant and silicagel column are 2��6:1 by volume;
Preferably, described alkanes eluent flow velocity is 0.2��2Bv/h;
Preferably, described acetone eluant flow velocity is 0.2��2Bv/h;
Preferably, the temperature of described concentration is 40 DEG C��100 DEG C;
Preferably, the pressure of described concentration is-0.03Mpa��-0.06Mpa;
Specifically, the method that the invention provides the yellow red separation of a kind of capsicum red pigment, the method comprises the following steps: a) Fructus Capsici granule and leaching agent is mixed in continuous way infuser, obtains pigment leachate; B) described pigment leachate is mixed with alcohols solvent in liquid-liquid continuous extraction device, slough spicy substance, obtain pigment and take off peppery leachate; C) described de-peppery pigment leachate and saturated aqueous common salt are mixed in liquid-liquid continuous extraction device, slough alcohols solvent residual; D) adopt wet method loading to separate through silica gel column chromatography the pigment leachate of elimination alcohols solvent, respectively obtain Fructus Capsici flavochrome and capsicum red pigment.
The method of the yellow red separation of capsicum red pigment provided by the invention, owing to employing continuous way liquid-liquid extractor so that de-peppery and dealcoholysis kind solvent process can operate continuously, and is suitable for the preparation of industrialization of capsicum red pigment; Additionally, the method of the yellow red separation of capsicum red pigment provided by the invention, in silica gel column chromatography separation process, the method directly adopting leachate wet method loading, silicagel column is enable to be applied in industrialized production, in industrialized production, obtain reddish yellow than low Fructus Capsici flavochrome and reddish yellow than high capsicum red pigment, it is achieved that the variation production of capsochrome simultaneously. Directly adopt the method for leachate wet method loading not report in the prior art, also do not provide relevant art enlightenment.
Additionally or preferably, the method that the invention provides the yellow red separation of a kind of capsicum red pigment, comprise the following steps:
A) by chilli powder and extractant hybrid extraction in continuous way infuser, pigment leachate is obtained;
B) pigment leachate is mixed with spicy-off agency in liquid-liquid continuous extraction device de-peppery, obtain de-peppery pigment extraction liquid;
C) de-peppery pigment leachate is mixed in liquid-liquid continuous extraction device elimination spicy-off agency with saturated aqueous common salt, obtain the pigment leachate of elimination spicy-off agency;
D) the pigment leachate of elimination spicy-off agency is carried out column chromatography for separation, respectively obtain the capsicum red pigment of the yellow and high reddish yellow ratio of Fructus Capsici of low reddish yellow ratio.
According to the present invention, first by maturation Fructus Capsici 30��50 DEG C of drying, pulverize, pelletize, obtain Fructus Capsici granule; Fructus Capsici granule delivers into inside continuous infuser through auger, in Fructus Capsici granule course of conveying, the extractant Homogeneous phase mixing sprayed with the pre-jet pipe of extractant, obtain mixed material, after described mixed material enters continuous infuser inside, making extractant be leached out by capsicum red pigment, obtain capsicum red pigment leachate, described pigment leachate is collected by the leachate catcher of continuous way infuser.
In the present invention, in Fructus Capsici granulation process, it is preferable that add the granulating and forming auxiliary agent based on dry paprika weighing scale 1 5%. Described granulating and forming auxiliary agent is preferably and comprises the cellulose repeating block shown in following formula (I):
This cellulosic molecular weight is 50,000-30 ten thousand. This cellulosic use, both ensure that pelletize requirement, has and ensure that granule has enough micropores for solvent extraction. The combination being mainly due in block two transconfigurations and a cis-structure.
Further preferably, this cellulose can be carried out surface modification, the cellulose of surface modification can be carried out, wherein by being carboxyl by the conversion of hydroxyl of cellulose surface, then make oligochitosan be covalently bound to the cellulose obtaining this surface modification on described carboxyl with oligochitosan.Described covalent bond includes peptide bond and/or imine linkage (C=N). Described hydroxyl can by being converted into carboxyl with potassium dichromate oxidation. Being covalently bound to by oligochitosan on described carboxyl can by using carbodiimide to carry out covalent bonding as connecting material. It is able to ensure that through so modified fiber and obtains higher Fructus Capsici particle porosity.
Before pelletizing, it is preferable that by Capsicum crushing to 50-150 order. The diameter of Fructus Capsici grain can be 1-6mm, it is preferable that 2-5mm.
Continuous way infuser of the present invention can be flat rotary extractor, loop type extractor, satellite type infusion device or crawler type infuser, the preferred flat rotary extractor of the present invention, extractant of the present invention can be the alkane containing 4��7 carbon, it is preferable that 6# solvent is as extractant. The spray temperature of described 6# solvent can be 40 DEG C��50 DEG C, and spray flux can be 1000L/h��1500L/h.
According to the present invention, described pigment leachate and alcohols spicy-off agency being mixed in liquid-liquid continuous extraction device, pigment leachate and alcohols spicy-off agency temperature can be 30 DEG C��50 DEG C, and pigment leachate flow can be 0.5m3/ h��1.5m3/ h, the flow of alcohols spicy-off agency can be 1m3/ h��3m3/ h, liquid-liquid continuous extraction device is pigment leachate at the middle and upper levels, and lower floor is alcohols solvent, and alcohols solvent can extract the capsaicin in pigment leachate, dihydro Capsaicin and drop the spicy substances such as dihydro Capsaicin. After elimination spicy substance, obtain de-peppery pigment leachate. Described alcohols material can be methanol, ethanol, propanol, isopropanol and butanol etc., and preferred alcohol of the present invention is as spicy-off agency.
According to the present invention, being mixed in liquid-liquid continuous extraction device with saturated aqueous common salt by described de-peppery pigment leachate, de-peppery pigment leachate flow can be 1m3/ h��3m3/ h, saturated common salt discharge can be 0.5m3/ h��1.5m3/ h, liquid-liquid continuous extraction device is pigment leachate at the middle and upper levels, and lower floor is saturated aqueous common salt, and saturated aqueous common salt can extract the alcohols solvent of residual in pigment leachate.
According to the present invention, the pigment leachate after elimination alcohols solvent is carried out column chromatography for separation. Obtain in pigment leachate after described elimination alcohols solvent and include the flavochrome components such as the red pigment component such as capsorubin, capsorubin and beta-carotene, cryptoxanthin, phylloxanthin. According to the present invention, described column chromatography is fixing can be silica gel, aluminium oxide, magnesium oxide etc. mutually. The preferred silica gel of the present invention is as the fixing phase of column chromatography, and silica gel specification used in the present invention can be 100 order��200 orders, 200 order��300 orders, it is preferable that 100 order��200 orders, the pigment extraction liquid of described elimination alcohols solvent with silica gel weight than preferred 1:5��10.
According to the present invention, the detailed process that silica gel column chromatography separates is: a) the pigment leachate of elimination alcohols solvent is directly gone up silicagel column and carries out adsorbing separation collection port effluent; B) upon adsorption saturated, adopt alkanes eluant that silicagel column carries out eluting, eluent is collected liquid with a) described port and is merged, and obtains Fructus Capsici flavochrome eluent, wherein comprises that beta-carotene, cryptoxanthin etc. be orange and xanthein. Being concentrated by described Fructus Capsici flavochrome eluent, the buff oily mater obtained is Fructus Capsici flavochrome; C) then with acetone, silicagel column is carried out eluting, obtain acetone eluant, acetone eluant includes the red pigments such as capsorubin and capsorubin.Being concentrated by described acetone eluant, the dark red oil material obtained is capsicum red pigment. The elimination alcohols solvent pigment extraction liquid sample loading mode continuous loading of preferred wet method of the present invention. Alkanes eluting solvent of the present invention can be the alkane containing 4��7 carbon, it is preferable that 6# solvent. 6# solvent and silica gel according to volume ratio preferably 2��4:1, acetone with silica gel according to volume ratio preferably 2��4:1,6# solvent and acetone elution speed all preferably 0.2��2Bv/h. Condensing mode of the present invention can be concentrating under reduced pressure and normal pressure concentration, the mode of the preferred concentrating under reduced pressure of the present invention, and pressure is-0.03Mpa��-0.06Mpa preferably, the temperature of concentration preferably 40 DEG C��100 DEG C.
Detailed description of the invention
Technical scheme is set forth below by way of instantiation.
In the method for the yellow red separation of capsicum red pigment provided by the invention, raw materials used, reagent, instrument etc. all can be buied by market.
Embodiment 1
Take Xinjiang maturation Fructus Capsici 3000Kg, dry, pulverize rear pelletize, adopt the continuous infuser of hoirzontally rotating that pigment leachate is obtained by extraction. By described pigment leachate and 70% ethanol in liquid-liquid extractor in 45 DEG C, mixing elimination spicy substance when 200r/min, pigment leachate flow is 1m3/ h, 70% ethanol flow is 2m3/ h, obtains de-peppery pigment leachate. Described de-peppery pigment leachate and saturated aqueous common salt mixs the ethanol of residual in elimination pigment extraction liquid in the 200r/min when, and taking off the peppery pigment extract flow amount that obtains is 1.8m3/ h, the flow of saturated aqueous common salt is 0.6m3/ h, obtains de-peppery pigment leachate. The mode that the pigment leachate of described elimination residual ethanol adopts continuous wet method loading carries out silica gel column chromatography separation with 1Bv/h flow velocity, collects lower port effluent. First carrying out eluting with 1500L6# solvent with 0.3Bv/h flow velocity, eluent is collected liquid with lower port and is merged, and obtains 6# eluate solvent. Concentrating under reduced pressure is adopted to obtain buff Fructus Capsici grease 59.1Kg described 6# eluate solvent. Then adopt 2000L acetone, with 0.3Bv/h flow velocity, silicagel column is carried out eluting, obtain acetone eluant. Concentrating under reduced pressure is adopted to obtain peony capsanthin ointment 109.7Kg described acetone eluant.
Embodiment 2
Take Gansu maturation Fructus Capsici 3000Kg, dry, pulverize rear pelletize, adopt the continuous infuser of hoirzontally rotating that pigment leachate Kg is obtained by extraction. By described pigment leachate and 70% ethanol in liquid-liquid extractor in 50 DEG C, mixing elimination spicy substance when 200r/min, pigment leachate flow is 1m3/ h, 70% ethanol flow is 1.5m3/ h, obtains de-peppery pigment leachate. Described de-peppery pigment leachate and saturated aqueous common salt mixs the ethanol of residual in elimination pigment extraction liquid in the 200r/min when, and taking off the peppery pigment leachate flow that obtains is 1.5m3/ h, the flow of saturated aqueous common salt is 0.5m3/ h, obtains de-peppery pigment leachate. The mode that the pigment leachate of described elimination residual ethanol adopts continuous wet method loading carries out silica gel column chromatography separation with 0.8Bv/h flow velocity, collects lower port effluent. First carrying out eluting with 1800L6# solvent with 0.5Bv/h flow velocity, eluent is collected liquid with lower port and is merged, and obtains 6# eluate solvent. Concentrating under reduced pressure is adopted to obtain buff Fructus Capsici grease 49.4Kg described 6# eluate solvent. Then adopt 2400L acetone, with 0.5Bv/h flow velocity, silicagel column is carried out eluting, obtain acetone eluant. Concentrating under reduced pressure is adopted to obtain peony capsanthin ointment 117.6Kg described acetone eluant.
Comparative example 1
Taking Xinjiang maturation Fructus Capsici 3000Kg, dry, pulverize rear pelletize, adopt the continuous infuser of hoirzontally rotating that pigment leachate is obtained by extraction, pigment leachate concentrating under reduced pressure obtains pigment ointment 246.5Kg, and pressure is-0.05Mpa. Described pigment ointment and 70% ethanol 600Kg being mixed, in 50 DEG C, 200r/min condition stirring 30min, rear insulation stands 1h, releases lower floor's ointment and is de-peppery pigment ointment 183.7Kg. Described de-peppery pigment ointment is mixed with 450Kg saturated aqueous common salt, stirs 30min in 200r/min condition, stand 1h afterwards, release lower floor's saturated aqueous common salt, obtain the pigment ointment 174.7Kg of de-ethanol residual. The pigment ointment of described de-ethanol is placed in silicagel column top, carries out the operation of chromatography. First carrying out affording 6# eluate solvent with 6000L6# solvent, flow velocity is 0.3Bv/h. Then adopting 5000L acetone to carry out eluting, obtain acetone eluant, flow velocity is 0.3Bv/h. Described 6# eluate solvent and acetone eluant are carried out concentrating under reduced pressure respectively, obtains Fructus Capsici flavochrome ointment 62.17Kg and capsicum red pigment ointment 110.8Kg.
Comparative example 2
Taking Xinjiang maturation Fructus Capsici 3000Kg, dry, pulverize rear pelletize, adopt the continuous infuser of hoirzontally rotating that pigment leachate is obtained by extraction, pigment leachate concentrating under reduced pressure obtains pigment ointment 273.1Kg, and pressure is-0.03Mpa. Described pigment ointment and 70% ethanol 800Kg being mixed, in 40 DEG C, 200r/min condition stirring 30min, rear insulation stands 1h, releases lower floor's ointment and is de-peppery pigment ointment 227.7Kg. Described de-peppery pigment ointment is mixed with 500Kg saturated aqueous common salt, stirs 30min in 200r/min condition, stand 1h afterwards, release lower floor's saturated aqueous common salt, obtain the pigment ointment 219.6Kg of de-ethanol residual. The pigment ointment of described de-ethanol is placed in silicagel column top, carries out the operation of chromatography. First carrying out affording 6# eluate solvent with 6500L6# solvent, flow velocity is 0.5Bv/h. Then adopting 6000L acetone to carry out eluting, obtain acetone eluant, flow velocity is 0.3Bv/h. Described 6# eluate solvent and acetone eluant are carried out concentrating under reduced pressure respectively, obtains Fructus Capsici flavochrome ointment 73.1Kg and capsicum red pigment ointment 138.3Kg.
Fructus Capsici flavochrome and capsicum red pigment prepared by embodiment and comparative example detect, absorbance, arsenic content, lead content, total organic solvent residual quantity, hexane residual quantity, acetone residue amount all detect according to the method for GB/10783-2008, and absorption ratio is the ratio of same capsicum red pigment solution A 470nm and A454nm. Testing result is as shown in table 1.
Capsicum red pigment testing result contrast prepared by table 1 embodiment 1��3 and comparative example.
Result according to table 1 is it can be seen that the Fructus Capsici flavochrome prepared of embodiment and comparative example and capsicum red pigment absorption ratio are close, but the yield of the Fructus Capsici flavochrome prepared of embodiment and capsicum red pigment is apparently higher than comparative example.
Result according to table 1 is it can be seen that the saturated extent of adsorption of embodiment silicagel column is substantially high and comparative example, it was shown that the content height of capsicum red pigment influences whether the silica gel saturated extent of adsorption to capsicum red pigment, thus having influence on the treating capacity of each batch.
Practical operation situation according to comparative example and embodiment, pigment ointment is directly placed in silicagel column top by comparative example, and in using 6# solvent elution process, the capsicum red pigment saturated extent of adsorption of silica gel is affected and is significantly greater than embodiment by flow velocity speed.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. the method for the yellow red separation of capsicum red pigment, it is characterised in that comprise the steps:
Step (1): Fructus Capsici granule and leaching agent are mixed in continuous way infuser, obtains pigment leachate;
Step (2): mixed in liquid-liquid continuous extraction device with alcohols solvent by described pigment leachate, slough spicy substance, obtains pigment and takes off peppery leachate;
Step (3): described de-peppery pigment leachate and saturated aqueous common salt are mixed in liquid-liquid continuous extraction device, sloughs alcohols solvent residual;
Step (4): the pigment leachate obtained after elimination alcohols solvent is directly gone up silicagel column and carries out chromatography collection port effluent;
Step (5): treat that silicagel column absorption is saturated, adopt alkane solvents to carry out eluting, eluent merges with the described port collection liquid of step (4) and concentrates to obtain Fructus Capsici flavochrome;
Step (6): adopt acetone that described silicagel column is carried out eluting, eluent concentration obtains capsicum red pigment.
2. extracting method according to claim 1, it is characterised in that described leaching agent is the alkane containing 4��7 carbon.
3. extracting method according to claim 1 and 2, it is characterised in that described infuser is flat rotary extractor, loop type extractor, satellite type infusion device or crawler type infuser.
4. extracting method according to claim 1 and 2, it is characterised in that described alcohols solvent is the alcohols solvent containing 1��4 carbon.
5. extracting method according to claim 1 and 2, it is characterised in that the pigment leachate described in step (2) and alcohols solvent mixed weight ratio are 1:1��7; De-peppery pigment leachate described in step (3) and saturated aqueous common salt mixed proportion are 1:1��7.
6. extracting method according to claim 1 and 2, it is characterised in that described silica gel column chromatography sample loading mode is the continuous loading of wet method.
7. extracting method according to claim 1 and 2, it is characterised in that the alkanes eluant described in step (5) is the alkane containing 4��7 carbon.
8. extracting method according to claim 1 and 2, it is characterised in that alkanes eluant described in step (5) and silicagel column are 2��6:1 by volume; Acetone eluant described in step (6) and silicagel column are 2��6:1 by volume.
9. extracting method according to claim 1 and 2, it is characterised in that described alkanes eluent flow velocity is 0.2��2Bv/h; Described acetone eluant flow velocity is 0.2��2Bv/h.
10. extracting method according to claim 1 and 2, it is characterised in that the temperature of described concentration is 40 DEG C��100 DEG C; The pressure of described concentration is-0.03Mpa��-0.06Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511017918.8A CN105647227A (en) | 2015-12-30 | 2015-12-30 | Method for separating red pigment from yellow pigment of paprika red pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511017918.8A CN105647227A (en) | 2015-12-30 | 2015-12-30 | Method for separating red pigment from yellow pigment of paprika red pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105647227A true CN105647227A (en) | 2016-06-08 |
Family
ID=56477321
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511017918.8A Pending CN105647227A (en) | 2015-12-30 | 2015-12-30 | Method for separating red pigment from yellow pigment of paprika red pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105647227A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106497138A (en) * | 2016-09-26 | 2017-03-15 | 河北东之星生物科技股份有限公司 | A kind of method for improving capsorubin content and absorption ratio |
| CN106631953A (en) * | 2016-12-29 | 2017-05-10 | 河南中大恒源生物科技股份有限公司 | Preparation method of beta-carotene in paprika |
| CN106866394A (en) * | 2017-03-08 | 2017-06-20 | 黄冈师范学院 | Capsorubin and preparation method thereof |
| CN109021613A (en) * | 2018-09-25 | 2018-12-18 | 云南瑞宝生物科技股份有限公司 | Capsicum red pigment and preparation method thereof |
| CN109744459A (en) * | 2018-11-27 | 2019-05-14 | 贵州红星山海生物科技有限责任公司 | A kind of extraction of capsochrome and sterilizing methods |
| CN111718598A (en) * | 2020-06-22 | 2020-09-29 | 河南中大恒源生物科技股份有限公司 | Production method of capsanthin with low polycyclic aromatic hydrocarbon |
| CN112029312A (en) * | 2020-08-20 | 2020-12-04 | 河北东之星生物科技股份有限公司 | Preparation method of capsorubin with high light absorption ratio and capsorubin with high content |
| CN114279992A (en) * | 2021-12-30 | 2022-04-05 | 广电计量检测（成都）有限公司 | Method for extracting and detecting yellow pigment in Huanggongfang pepper |
| CN115381094A (en) * | 2022-08-18 | 2022-11-25 | 河南中大恒源生物科技股份有限公司 | Low-odor water-soluble copper chlorophyll and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059742A (en) * | 1990-09-11 | 1992-03-25 | 周建功 | Extract capsochrome and peppery plain processing method by capsicum |
| CN101338080A (en) * | 2008-05-05 | 2009-01-07 | 苏州市兴科现代中药工艺装备开发有限公司 | Method for removing capsaicin in production process of capsanthin pigment |
| CN101760039A (en) * | 2009-09-26 | 2010-06-30 | 美科尔(河北)生物科技有限公司 | Method for removing capsaicin during production process of capsicum red pigment |
| CN101831198A (en) * | 2010-05-27 | 2010-09-15 | 文雁君 | Preparation method of capsanthin |
| CN101870825A (en) * | 2010-07-19 | 2010-10-27 | 河北瑞德天然色素有限公司 | Technique method for extracting capsicum red pigment after capsicum powder granulation |
| CN103013163A (en) * | 2012-12-13 | 2013-04-03 | 晨光生物科技集团股份有限公司 | Production method of high-color-value capsanthin pigment |
-
2015
- 2015-12-30 CN CN201511017918.8A patent/CN105647227A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059742A (en) * | 1990-09-11 | 1992-03-25 | 周建功 | Extract capsochrome and peppery plain processing method by capsicum |
| CN101338080A (en) * | 2008-05-05 | 2009-01-07 | 苏州市兴科现代中药工艺装备开发有限公司 | Method for removing capsaicin in production process of capsanthin pigment |
| CN101760039A (en) * | 2009-09-26 | 2010-06-30 | 美科尔(河北)生物科技有限公司 | Method for removing capsaicin during production process of capsicum red pigment |
| CN101831198A (en) * | 2010-05-27 | 2010-09-15 | 文雁君 | Preparation method of capsanthin |
| CN101870825A (en) * | 2010-07-19 | 2010-10-27 | 河北瑞德天然色素有限公司 | Technique method for extracting capsicum red pigment after capsicum powder granulation |
| CN103013163A (en) * | 2012-12-13 | 2013-04-03 | 晨光生物科技集团股份有限公司 | Production method of high-color-value capsanthin pigment |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106497138A (en) * | 2016-09-26 | 2017-03-15 | 河北东之星生物科技股份有限公司 | A kind of method for improving capsorubin content and absorption ratio |
| CN106631953A (en) * | 2016-12-29 | 2017-05-10 | 河南中大恒源生物科技股份有限公司 | Preparation method of beta-carotene in paprika |
| CN106631953B (en) * | 2016-12-29 | 2019-01-22 | 河南中大恒源生物科技股份有限公司 | The preparation method of beta carotene in a kind of capsicum |
| CN106866394A (en) * | 2017-03-08 | 2017-06-20 | 黄冈师范学院 | Capsorubin and preparation method thereof |
| CN109021613A (en) * | 2018-09-25 | 2018-12-18 | 云南瑞宝生物科技股份有限公司 | Capsicum red pigment and preparation method thereof |
| CN109744459A (en) * | 2018-11-27 | 2019-05-14 | 贵州红星山海生物科技有限责任公司 | A kind of extraction of capsochrome and sterilizing methods |
| CN111718598A (en) * | 2020-06-22 | 2020-09-29 | 河南中大恒源生物科技股份有限公司 | Production method of capsanthin with low polycyclic aromatic hydrocarbon |
| CN112029312A (en) * | 2020-08-20 | 2020-12-04 | 河北东之星生物科技股份有限公司 | Preparation method of capsorubin with high light absorption ratio and capsorubin with high content |
| CN114279992A (en) * | 2021-12-30 | 2022-04-05 | 广电计量检测（成都）有限公司 | Method for extracting and detecting yellow pigment in Huanggongfang pepper |
| CN114279992B (en) * | 2021-12-30 | 2024-03-22 | 广电计量检测（成都）有限公司 | Extraction and detection method of yellow pigment in yellow Gong Jiao |
| CN115381094A (en) * | 2022-08-18 | 2022-11-25 | 河南中大恒源生物科技股份有限公司 | Low-odor water-soluble copper chlorophyll and preparation method and application thereof |
| CN115381094B (en) * | 2022-08-18 | 2023-10-24 | 河南中大恒源生物科技股份有限公司 | Low-odor water-soluble copper chlorophyll and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105647227A (en) | Method for separating red pigment from yellow pigment of paprika red pigment | |
| CN100537586C (en) | Method for producing high purity jasminoidin and high color number gardenia yellow pigment | |
| CN102276679B (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN106588616B (en) | A kind of preparation method of curcumin | |
| CN110283048A (en) | The preparation method of cannabidiol crystal | |
| CN102659652B (en) | Solid phase extraction method for extracting total astaxanthin from haematococcus pluvialis | |
| CN102228499B (en) | Method for separating naphthoquinone active ingredients from sinkiang arnebia root | |
| CN102408320B (en) | Method for extracting and separating curcumin and curcuma oil from carcuma longa | |
| CN103265519B (en) | The method of Folium Myricae rubrae proanthocyanidin is prepared in a kind of separation | |
| CN107459838B (en) | Subcritical abstraction combines the method for preparing medlar carotenoid class natural pigment with membrane separating and purifying concentration | |
| CN102500134B (en) | Preparation method and application of molecularly imprinted solid phase extraction small column for separating pyrethroid pesticide | |
| CN110776449B (en) | Industrial method for extracting lutein and quercetagetin | |
| CN101962486A (en) | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato | |
| CN110105257A (en) | A kind of synchronous industrial method for extracting lutein and quercetagetin | |
| CN105061529A (en) | Extraction process of mulberry anthocyanin | |
| CN103664855B (en) | A kind of high purity oligomer LSPC preparation method | |
| CN102558902B (en) | Process for extracting gardenia yellow from gardenia | |
| CN111848362A (en) | Method for preparing high-purity cannabidiol by combining ultrasonic extraction with dynamic axial compression column system | |
| CN105153253A (en) | Purple sweet potato anthocyanin extraction process | |
| CN100582102C (en) | Process for preparing methylation catechin by tea | |
| CN102432656B (en) | Method for extracting and purifying cordycepin from Cordyceps militaris sporophore | |
| CN101704729A (en) | Method for extracting resveratrol and polydatin in grape seeds | |
| CN101838178A (en) | Preparation method of lycopene | |
| CN112999252B (en) | Industrial method for continuously extracting high-content marigold flavone | |
| CN104926904B (en) | A kind of method of extraction purification cordycepin in mycoderma from Cordyceps militaris |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160608 |
|
| RJ01 | Rejection of invention patent application after publication |